• Title/Summary/Keyword: ether extraction

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Synthesis and Small Animal Brain PET Study of a Serotonin Receptor Radiotracer, 18F-Mefway (세로토닌 5-HT1A수용체 방사성 추적자 18F-Mefway의 합성과 소동물 뇌 PET 연구)

  • Ahn, Sung-Min;Hong, Tae-Kee;Ryu, Young-Hoon;Choi, Jae-Yong;Kim, Sung-Chul
    • The Journal of the Korea Contents Association
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    • v.9 no.11
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    • pp.262-270
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    • 2009
  • $^{18}F$-mefway has been developed as radioligand for serotonin receptor 5-$HT_{1A}$. The object of this study was to obtain the mefway precursor with the higher yield than previous method and to identify whether $^{18}F$-mefway can bind to 5-$HT_{1A}$ or not. from microPET imaging of small animal brain. Precursor was prepared by a modification of the reported procedure then [$^{18}F$] labeling was performed by adding $^{18}F$ ion at $130^{\circ}C$ in the hot cell for 30min. After purification of reaction mixture using alumina Sep-pak and HPLC, microPET images of small animal brain were determined. The chemical yield of precursor was increased from 9% to 34% using oxalyl chloride and LAH/diethylether. We synthesized a precursor which was successfully labeled with no-carrier-added $^{18}F$-by new synthetic route. This research suggest that $^{18}F$-mefway will be used a radiopharmaceutical for evaluation of central nerve system disorder as imaging a gent for 5-$HT_{1A}$ receptor.

Anticancer Activity of Acanthopanax trifoliatus (L) Merr Extracts is Associated with Inhibition of NF-κB Activity and Decreased Erk1/2 and Akt Phosphorylation

  • Wang, Hua-Qian;Li, Dong-Li;Lu, Yu-Jing;Cui, Xiao-Xing;Zhou, Xiao-Fen;Lin, Wei-Ping;Conney, Allan H.;Zhang, Kun;Du, Zhi-Yun;Zheng, Xi
    • Asian Pacific Journal of Cancer Prevention
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    • v.15 no.21
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    • pp.9341-9346
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    • 2014
  • Acanthopanax trifoliatus (L) Merr (AT) is commonly used as an herbal medicine and edible plant in some areas of China and other Asian countries. AT is thought to have anticancer effects, but potential mechanisms remain unknown. To assess the anticancer properties of AT, we exposed prostate cancer cells to AT extracts and assessed cell proliferation and signaling pathways. An ethanol extract of AT was suspended in water followed by sequential extraction with petroleum ether, ethyl acetate and n-butanol. PC-3 cells were treated with different concentrations of each extract and cell viability was determined by the MTT and trypan blue exclusion assays. The ethyl acetate extract of the ethanol extract had a stronger inhibitory effect on growth and a stronger stimulatory effect on apoptosis than any of the other extracts. Mechanistic studies demonstrated that the ethyl acetate extract suppressed the transcriptional activity of NF-${\kappa}B$, increased the level of caspase-3, and decreased the levels of phospho-Erk1/2 and phospho-Akt. This is the first report on the anticancer activity of AT in cultured human prostate cancer cells. The results suggest that AT can provide a plant-based medicine for the treatment or prevention of prostate cancer.

Multiple Determinations of Trichloroethylene Metabolites in a Concurrent Biological Media using High Performance Liquid Chromatography Coupled with Tandem Mass Spectrometry (HPLC-MS/MS를 이용한 트리클로로에틸렌 대사산물의 다중 분석법 확립)

  • Ahn, Youngah;Kho, Younglim;Lee, Seungho;Shin, Mi-Yeon;Jeon, Jung Dae;Kim, Sungkyoon
    • Journal of Environmental Health Sciences
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    • v.40 no.2
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    • pp.114-126
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    • 2014
  • Objectives: We aimed to develop a measurement method of five metabolites of trichloroethylene (TCE) in a concurrent biological sample, e.g., trichloroacetic acid (TCA), dichloroacetic acid (DCA), S-(1,2-dichlorovinyl) glutathione (DCVG), S-(1,2-dichlorovinyl)-L-cysteine (DCVC), and N-Acetyl-S-(1,2-dichlorovinyl)-L-cysteine (NAcDCVC) and to validate the method before application to pharmacokinetic study. Methods: TCE metabolites were simultaneously analyzed using high performance liquid chromatography coupled with electrospray ionization mass spectrometry (HPLC-ESI-MS/MS) with as little as 50 ${\mu}L$ of serum and urine. DCA, TCA and NAcDCVC were extracted with diethyl ether, while DCVC and DCVG were extracted by solid phase extraction. This method was validated according to the guidelines for bioanalytical method validation of the Korean National Institute of Toxicological Research. Then, we determined the five metabolites in five strains of mice at 24 hr after exposure to 1 g TCE /kg body weight. Results: The limits of detection for the five metabolites in biological samples ranged from 0.001 to 0.076 nmol/mL, which is comparable to or better than those previously reported. Most calibration curves showed good linearity ($R^2=0.99$), and between-batch variation was less than 20% expressing acceptable robustness and reproducibility. Using this method, we found TCA and DCA were detected in all test mice at 24 hr after the oral administration while NAcDCVC and DCVC were detected in some strains, which showed strain-dependent metabolism of TCE. Conclusions: The present method could provide robust and accurate measurements of major key metabolites of TCE in biological media, which allowed concurrent analysis of TCE metabolism for limited amounts of biospecimens.

The Effect of Dispersion Medium on Intensity of Volatile Flavor Components and Recovery of Essential Oil from Capsella bursa-pastoris by Steam Distillation (수증기 증류시 분산매의 조성이 냉이의 휘발성 향기성분의 강도 및 정유 회수율에 미치는 영향)

  • Choi, Hyang-Sook;Lee, Mie-Soon
    • Korean Journal of Food Science and Technology
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    • v.28 no.5
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    • pp.827-833
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    • 1996
  • Along with the increased necessity for an efficient utilization of Korean wild edible plants growing in fields and mountains, attempts were made to investigate the patterns of flavor changes accompanied hy various conditions of dispersion medium. The effect of various pH values and concentration of sucrose or NaCl of dispersion medium on volatile flavor patterns was investigated to evaluate the applicability of flavor components extracted from Capsella bursa-pastoris for food industry. Essential oils from this wild plant were isolated by simultaneous steam distillation-extraction (SDE) method using diethyl ether as solvent. Concentrated samples were analyzed s chromatography (GC) and combined gas chromatography-mass spectrometry (GC-MS). Most volatile flavor components of Capsella bursa-pastoris showed good recovery when steam distilled at pH 7 by SDE method. Increasing concentration of sucrose and 15% by NaCl, resulted in greater numbers of identified flavor components from Capsella bursa-pastoris.

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Rapid Gas Chromatographic Screening of Vegetable Oils for Free Fatty Acids (기체크로마토그래피법에 의한 식물성 유지내 유리 지방산의 신속한 스크리닝)

  • Kim, Jung-Han;Kim, Kyoung-Rae;Chai, Jeong-Young;Oh, Chang-Hwan;Park, Hyung-Kook
    • Korean Journal of Food Science and Technology
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    • v.25 no.4
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    • pp.373-378
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    • 1993
  • A rapid gas chromatographic profiling method for the simultaneous analysis of free fatty and other acids was applied to vegetable oils. Oil samples were dissolved in dichloromethane and the free acids were extracted with saturated $NaHCO_3$ solution. The aqueous extract was acidified and then loaded onto the Chromosorb P column for the extraction. The acids were eluted with diethyl ether selectively from Chromosorb P column and were treated with triethylamine to prevent the losses of volatile acids. Several long chain fatty acids were detected from soybean oil, rice-bran oil, sesame oil and perilla oil. Various organic acids including odd number fatty acids were detected in crude oil, especially sesame oil. Arachidic acid from perilla oil and vanillic acid from sesame oil, which were not reported before were detected. The content ratio of free linoleic acid to oleic acid was $1.02{\sim}1.18$, which was similar to the reported data. When the GC profile of organic acids were simplified to their corresponding retention index spectra of bar graphical forms, they presented characteristic pattern of each vegetable oil that can be quickly recognized.

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Development and Validation of an HPLC Method for the Pharmacokinetic Study of Dipyridamole in Human (디피리다몰 체내동태 연구를 위한 혈청 중 디피리다몰의 HPLC 정량법 개발 및 검증)

  • Cho, Hea-Young;Kang, Hyun-Ah;Moon, Jae-Dong;Choi, Hoo-Kyun;Lee, Yong-Bok
    • Journal of Pharmaceutical Investigation
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    • v.36 no.1
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    • pp.45-51
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    • 2006
  • A rapid, selective and sensitive reversed-phase HPLC method for the determination of dipyridamole in human serum was developed, validated, and applied to the pharmacokinetic study of dipyridamole. Dipyridamole and internal standard, loxapine, were extracted from human serum by liquid-liquid extraction with diethyl ether and analyzed on a Nova Pak $C_{I8}$ column with the mobile phase of 40 mM ammonium acetate:methanol:acetonitrile (35:35:30)(v/v/v, pH 7.8). Detection wavelength of 280 nm and flow rate of 1.0 mL/min were fixed for the study. The assay robustness for the changes of mobile phase pH, organic solvent content, and flow rate was confirmed by $3^3$ factorial design using a fixed dipyridamole concentration (50 ng/mL) with respect to its peak area and retention time. And also, the ruggedness of this method was investigated at three different laboratories using same quality control (QC) samples. This method showed linear response over the concentration range of 2-2000 ng/mL with correlation coefficients greater than 0.999. The lower limit of quantification using 0.5 mL of serum was 2 ng/mL, which was sensitive enough for pharmacokinetic studies of dipyridamole. The overall accuracy of the quality control samples ranged from 103.94 to 105.86% for dipyridamole with overall precision (% C.V.) being 4.60-11.49%. The relative mean recovery of dipyridamole for human serum was 97.64%. Stability studies showed that dipyridamole was stable during storage, or during the assay procedure in human serum. The peak area and retention time of dipyridamole were not significantly affected by the changes of mobile phase pH, organic solvent content, and flow rate under the conditions studied. This method showed good ruggedness (within 15% C.V.) and was successfully used for the analysis of dipyridamole in human serum samples for the pharmacokinetic studies of orally administered Dimor tablet (75 mg as dipyridamole) at three different laboratories, demonstrating the suitability of the method.

Analysis of Volatile Flavor Components from Perilla frutescens var. acuta and Sensory Evaluation as Natural Spice (소엽의 휘발성 향미성분 분석 및 향신료로서의 관능적 평가)

  • 정미숙;이미순
    • Korean journal of food and cookery science
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    • v.16 no.3
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    • pp.221-225
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    • 2000
  • This study was conducted to investigate the usefulness of Perilla frutescens var. acuta as a natural spice. Volatile flavor components of dried Perilla frutescens var. acuta were extracted by supercritical fluid extraction method using diethyl ether as solvent. Essential oils were analyzed by gas chromatography (GC) and combined gas chromatography-mass spectrometry (GC-MS). Identification of volatile flavor components was based on the RI of GC and mass spectrum of GC-MS. A total of 24 components, including 4 hydrocarbons, 3 aldehydes, 8 alcohols, 4 esters, 3 acids and 2 miscellaneous components were identified in the essential oils. L-Perillaldehyde was found to be the major volatile flavor component of dried Perilla frutescens var. acuta. The masking effects of Perilla frutescens var. acuta on meaty and fishy flavor were measured by sensory evaluation. Meaty flavor was significantly reduced with the addition of 0.05%, 0.1%, and 0.2% Perilla frutescens var. acuta. The addition of 0.1% and 0.2% powdered Perilla frutescens var. acuta also reduced the fishy flavor of mackerel.

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Analysis of Volatile Flavor Components from Zanthoxylum schinifolium and Sensory Evaluation as Natural Spice (산초의 휘발성 향미성분 분석 및 향신료로서의 관능적 평가)

  • 이미순;정미숙
    • Korean journal of food and cookery science
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    • v.16 no.3
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    • pp.216-220
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    • 2000
  • Volatile flavor components in the fruits of dried Zanthoxylum schinifolium were extracted by supercritical fluid extraction method using diethyl ether as solvent. Essential oils were analyzed by gas chromatography (GC) and combined gas chromatography-mass spectrometry (GC-MS). Identification of volatile flavor components was based on the RI of GC and mass spectrum of GC-MS. A total of 30 components, including 6 hydrocarbons, 4 aldehydes, 8 alcohols, 5 esters, 4 acids and 3 miscellaneous components were identified in the essential oils. Geranyl acetate, ${\beta}$-phellandrene, D-limonene and citronellal were found to be major volatile flavor components in fruits of dried Zanthoxylum schinifolium. The masking effects of Zanthoxylum schinifolium on meaty and fishy flavor were measured by sensory evaluation to investigate the usefulness of Zanthoxylum schinifolium as a natural spice. Meaty flavor was significantly reduced with the addition of 0.05% and 0.1% Zanthoxylum schinifolium. And the addition of 0.l% powdered Zanthoxylum schinifolium also reduced the fishy flavor of mackerel.

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The Oxidative Stability of Solvent Extracts of Sea Tangle Powder(STP)and Maejakgwa Made with STP (다시마 용매추출물과 다시마 분말 첨가에 의한 매작과의 산화안정성)

  • Park, Bock-Hee;Cho, Hee-Sook;Kim, Kyung-Hee;Kim, Sun-Sook;Kim, Hyun-A
    • Korean journal of food and cookery science
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    • v.24 no.4
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    • pp.452-459
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    • 2008
  • The purpose of this study was to investigate the antioxidative effects of Sea tangle powder(STP) solvent extracts as well as Maejakgwa made with STP. The STP solvent extracts were added to soybean oil at a quantity of 0.05%. The solvents used for extraction were methanol, ethanol, ethyl acetate, and petroleum ether. Soybean oil without added STP was used as a negative control, and soybean oil samples containing 0.02% butylated hydroxy toluene(BHT) and $\alpha$-tocopherol were used as positive control, respectively. Each sample was stored at $50^{\circ}C$ for 30 days. The oxidation levels of these samples were determined by measuring their acid values, peroxide values, and thiobarbituric acid(TBA) values. The soybean oil samples containing the STP extracts had lower oxidation levels than both the negative control and $\alpha$-tocopherol positive control, and the sample containing the 0.05% methanol extracts had the lowest oxidation. According to the Rancimat method, the methanol extract(320 min) and ethanol extract(316 min) demonstrated longer induction periods as, compared to the control(253 min), $\alpha$-tocopherol(255 min), and BHT(309 min) samples. For the Maejakgwa, acid values increased over the storage period, however, the samples made with STP had lower values than the control group. Peroxide values increased rapidly for 30 days and then decreased. The TBA values of the Maejakgwa samples made with 3% and 9% STP were lower than those of the 15% STP sample and the control. In conclusion, the oxidative stability of soybean oil containing solvent extracts of STP and Maejakgwa made with STP were increased.

Volatile Flavor Components of Commelina communis L. as Influenced by Drying Methods (닭의장풀의 건조방법에 따른 휘발성 향기성분)

  • Lee, Mie-Soon;Choi, Hyang-Sook
    • Korean Journal of Food Science and Technology
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    • v.27 no.3
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    • pp.380-386
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    • 1995
  • An attempt was made to determine the effects of drying methods including shady air drying, presteamed and shady air drying, microwave drying, and freeze drying on the volatile flavor components with Commelina communis L.. Essential oils from the samples were isolated by simultaneous steam distillation-extraction(SDE) method using diethyl ether as solvent. Concentrated samples were analyzed by gas chromatography(GC) and combined gas chromatography-mass spectrometry(GC-MS). Respective 29, 47, 36, and 24 volatile flavor components were identified in shady air dried samples, presteamed and shady air dried samples, microwave dried samples, and freeze dried samples. The kinds and amounts of volatile flavor components were evidently depended upon the drying methods. 6,10,14-trimethylpentadecanone was regarded as the most abundant component in shady air dried samples, 6,10,14-trimethyl-2-pentadecanone in presteamed and shady air dried samples, neophytadiene in microwave dried samples, and ethyl acetate in freeze dried samples.

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